Table of Content *

Confidential Proposal Summary *

Scientific/technical objectives and innovation *

Project Workplan *

WP1: Project Management *

WP2: Methodology development *

WP3: Expert system implementation *

WP4: Instrument installation *

WP5: Samples preparation and qualification *

WP6: Analysis and comparison of qualified samples *

WP7: Problem solving of process engineering *

WP8: Dissemination *

Gantt diagram/man power *

Forms *

In this project we propose the development of an instrument for X-Ray diffractometry and X-Ray reflectivity dedicated to measurements of film thickness, surface and interface roughness, density, crystalline phase, texture and residual stress of supported thin films dedicated to microelectronics materials and devices.

The design of such instrument will address the need of a non-destructive, fast and user friendly technique able to characterise thin films for the microelectronics industry. The project aims to provide a tool that overcomes the intrinsic limitation that ellipsometry has on ultra-thin (few nanometers range) film thickness measurements, to provide additional fundamental information on thin films and to deliver them in a user friendly form facilitating development of new processes in microelectronics. The instrument that we propose will allow to gain a finer control over the production steps of microelectronics devices improving reliability and minimising waste. Moreover, this project will bring European instrument manufacturers in close contact with European semiconductor industries, with benefits on both sides. The research to be carried out will develop new and improved instrumentation and measuring system, including software, with the capabilities required by the end-users. It will be part of the Generic Activity in the Competitive and Sustainable Growth Program, addressing objective 6.1-Insrumentation.

The project will be organised as follow:

• X-Ray diffractometry and reflectivity will be integrated in a single instrument equipped with a small spot collimator to achieve high lateral resolution. The software interface responsible for data collection will be optimised to achieve maximum efficiency in data collection.
• An expert system will be defined where appropriate computing algorithm for data interpretation and a friendly graphical user interface will be optimised according to the need of the end user.
• Instrument will be installed, his specification will be verified
• The instrument will be tested in order to verify performance and easiness to operate. In this phase minor modification of software/hardware will be implemented based on feedback from the users. Standard silicon oxides deposited on silicon will be prepared. Film thickness will be measured with X-Ray reflectivity and comparatively with other techniques. Ferroelectric thin films of modified lead titanate (PZT) and strontium bismuth tantalate (SBT) will be prepared on different substrates. Their texture and stress/strain will be measured. Thickness of the layers of the stack (Pt, TiO₂ or Ti buffers) will be also determined, since it affects the development of texture in these films. Titanium silicides, aluminium and copper films will be prepared as uniform films and as test pattern as well. Texture, microstructure stress/strain will be evaluated with the new instrumentation.
• A competitive comparison between the technique proposed and the techniques currently used will be performed. The same samples described in the previous part will be prepared and analysed. Thin films thickness will be measured by means of ellipsometry. For ferroelectric thin films, the ferropiezoelectric behaviour will be compared to the texture results in order to obtain correlation. Stress/strain on test pattern and uniform films will be tested by means of Raman spectroscopy and by curvature measurements. A comparison chart will be made to critically analyse the advantages and disadvantages of the new approach.
• Dissemination of results will be performed through demonstrations done on leading edge thematic meetings between the industrial users, through participation in international congress and by organisation of a workshop.
• The team will include three research groups from three different European countries, two instrument manufacturers from two countries and one user industry, representing three European countries at total. The instrument will be placed inside one of the research institution, which will be responsible for the project co-ordination and management of the relation between users and manufacturers. Two research institutions will be involved in software development, algorithm optimisation and testing. The other research institutions and the industrial user will prepare samples and perform control and comparative analysis. This project will deliver a valuable tool for thin film characterisation, tailored for the needs of microelectronics industry, but extensible to other fields. A non-destructive and easy-to-use method for precise thickness measurements will be proposed as a new standard. The instruments modified and integrated according to the feedback from users will eventually be commercialised on the basis of an agreement between the two manufacturers.

Microelectronic industry is employing ellipsometry as the accepted methodology to obtain film thickness and normal X-ray diffraction (Bragg-Brentano geometry or texture instruments) to characterise qualitatively texture and phase content. Some advanced research centres (not industrial) are starting to use the reflectivity method to characterise films with thickness lower than the acceptable range for ellipsometry, but the technique requires a special apparatus for grazing angle diffraction and a senior researcher expert of the field able to deal with the basic equations of reflectivity and with sufficient experience to perform the correct experiment. Nevertheless this methodology gives more accurate results than ellipsometry and is not limited by the small thickness of the film or by a multilayer structure.

The quantification of texture is more complicated from the methodological point of view. The traditional approach, based on the development of the orientation distribution function in a series of spherical harmonics, provides with quantitative information of the texture of the material after the analysis of the X-ray results. Although this approach is interesting for the easy prediction of the macroscopic properties, it is not for the sharp textures generally encountered in the electronic thin film field. As a result, the current practice in both industry and research laboratories is to analyse only qualitatively the film texture omitting any orientation distribution function (o.d.f.) computation. Nowadays, only few laboratories are starting to use a particular methodology for texture analysis based on entropy algorithms and discrete approximation of the o.d.f. and to test it to texture characterisation of thin films. The methodology requires a particular instrument set-up and it has not been automated for general users.

Residual stress analysis in thin film has been investigated extensively, from a methodological point of view, but due to its inter-relations with the strong texture of these structures, the techniques commercially available are not acceptable for the microelectronics industry. Researchers have created some sophisticated methodologies to overcome the problem but these are time consuming because they require a first determination of the texture, a subsequent elastic tensor homogenisation and lastly a modified measurement and approach for stress determination. This takes one week of measurements and analysis and, neglecting the texture to accelerate the process, will lead to errors of 3-500%. The practical result is that the residual stress state and the o.d.f. are not analysed out of very few academic research centres.

In summary, most of the physical properties of thin films are accessible to advanced laboratories but not to films makers especially in industry, because of the special instrumentation set-up and scientific background required. Even more limiting is the fact that the total amount of time (both instrument and operator/researcher) necessary for a complete control is very far from any industry standard. Most of the time is too much also for academic research purposes unless the importance of the result will justify the work.

The proposed approach will use a unique apparatus and experimental method unified for all the analyses mentioned above. By this method the instrument and operator time can be decreased noteworthy and also standardised for automatic collection. This can be accomplished by a special apparatus able to collect diffraction spectra at different tilting angles of the sample. The instrument must be equipped with a goniometer able to cover the entire pole figure (PF) angles in a half sphere space, a sample holder for large wafer mounting and a curved position sensitive detector collecting an entire diffraction spectrum at one time. The minimum tilting angle number necessary to the complete analysis will be chosen by the expert system based on some new algorithms and PF coverage optimisations. Spectra analysis will be processed by the expert system by calculating all interesting physical properties simultaneously. This will be done through the integration of a Rietveld (full pattern analysis), WIMV (for texture, see Wenk et al., 1994), residual stress, reflectivity and line-broadening (microstructure) methods in a unique non-linear least square fitting of the data. This will lead to an improved analysis, especially for the texture-stress-crystal structure effect separation. Also the integration of the reflectivity analysis with the crystal structure refinement will permit to obtain the inner structure of a multi-layer or single layer instead of its simple thickness. The thickness also will be very important for the residual stress computation.

The overall technique can be fully automated both from the point of view of the experimental data collection than for the final analysis. Also through the implementation of the expert system, integrating experiment and analysis, deficiencies in the PF coverage or missing data can be identified soon and repaired without invalidating the entire process.

Overall optimisation of the technique will lead to a consistent reduction of the analysis time allowing the methodology to be validated for industrial and quality control needs.

Some of these integrated techniques have been already tested by some of the laboratories participating to the project to ensure feasibility. E.g. the integration of texture and residual stresses analyses, or crystal structure and microstructure, or crystal structure and texture. Some tests have been performed also to study the validity of an automatic approach to the analysis with results better than the author’s expectations.

In summary, the most innovative points of this expert system for general non-destructive analysis of thin film are:

• Analysis of texture, structure, microstructure, quantitative phase content, surface and interface roughness, densities, thickness and residual stress in a single step using a single experiment and apparatus
• Integration of the measurement and analysis for time saving and better reliability of the results using an expert system.
• Automatic mode of operations from the data collection experiment to the final analysis. Operator intervention is reduced to minimum,
• Output of the program in term of physical properties and characteristics directly usable by the end user.
• Analysis of macro or micro-areas through the use of a capillary collimator. An entire wafer can be scanned trough the measurement.
• The expert system program GUI (graphical user interface) will be written in the object oriented language Java allowing it to run on any platform and trough the internet for remote control of the system.
• The core program will have a plug-in structure allowing expert users to introduce new features in the system without a knowledge of the inner structure and the need to recompile the program,

Some testing has been done to integrate in pair some of the methodologies (texture and stress, microstructure and crystal structure, texture and crystal structure/microstructure) at a laboratory level and the feasibility and benefits of the procedure have been demonstrated. Not all the aspects have had equal opportunity to be tested by the proposers for real applicability to film for microelectronic. Even if theory and experience lead to very optimistic expectations, only the real testing of the new instrument and system can give an idea of the accuracy attainable by the new integrated methodology especially for the integration of diffraction and reflectivity experiments, never done or proposed until now.

The main unknown points to test during the project development are:

• Investigation of structure of different layer and multi-layers in addition to thickness using both diffraction and reflectivity measurements at the same time.
• Possibility to investigate unknown structures with strong texture.
• Assessment of the general procedure and accuracy obtainable.
• Feasibility of a rapid quality control system using a reduced subset of analysis for on-line non-destructive check.
• Feasibility of a reduced cost apparatus for general analysis with simplified geometry.
• All these technical approaches will need compromises that will have to be dealt with on the practical point of view. And this will depend on the sample characteristics. Then the experimental set-up itself will need to be changed in configuration, adapted to several different samples (example: for roughness-dependent properties, reflectometry is a method of choice, but needs a thin collimation (typically 50-100 microns), which is not adequate for texture measurements)
• Difficulty to combine the need for a reasonable analysis time with not too an expensive apparatus that will limit the possibility of a good diffusion. This is mainly connected with the measuring time because the computing time for the analysis is rapidly decreasing with today new fast computers and can be dramatically increased through the implementation of a distributed computing system. This can be quite easily done using the Java implementation of the analysis program.

The project plan: the activities of monitoring and controlling the project will be based on the project plan (Gantt). An operational project plan will be prepared complete with resource allocation for each member of the partner project teams while preparing the project technical annex.

This will be used to monitor the information in the progress report preparation procedure (see next paragraph), that will be monitored by enabling effective corrective re-planning of a project level where corrective action within the bounds of workpackage proves impossible. This will enable consideration to be given to the critical path, available slack times between related tasks, dependencies between tasks and resource availability when carrying out the re-scheduling activities. It will also be used as a tool for providing the EU with a rapid project progress graphical overview at any stage of the project, and will be provided together with the project progress report.

Partners responsible for workpackages will also use the project plan as their own planning tool. They will be responsible for the monitoring, control and management of the component tasks. Dependencies between components of their workpackages and components of other workpackages will be evidenced by the project plan, and assure that their own planning activities respect that of others.

Progress Report: these reports will be provided to the EU every two or three months (timing to be agreed with the EU). These reports will be used first and for most to ensure monitoring of the project by involving the partners responsible for workpackages in its production.

The progress report will give workpackage and task planned (from original project plan) finish and start dates against expected (changed expectancy) finish and start dates. In the case of delays explanations will be provided together with corrective actions to be taken. The same will be done for deliverables. Where the partner responsible for a workpackage is unable to supply adequate corrective actions, responsibility is past to the project co-ordinator. The report will also compare resource usage between expected and actual providing explanations of differences.

T2.1: Methodologies definitions

The most suitable methodologies for the required analyses and integration on the expert system will be selected. Criteria for selection will be the accuracy of results, suitability for integration in the automated system and flexibility of the methodology respect to the needs.

The methodologies to be selected for the analysis will concern the following fields: thickness and layer structure, film texture and residual stresses, crystal structure, planar and line defect density. Some additional theories for film properties computation from the analysed characteristics are to be selected mainly in the area of homogenisation techniques.

T2.2: Methodologies integration

The selected methodologies will be modified to be suitable for integration in the whole system. The synergy of the approach will allow also to add some more features not analysable by the separated theories. Especially the integration of the reflectivity analyses for film thickness determination with a multi-layer approach and the structural diffraction analysis will permit to obtain the inner structure of different film layers. Some integration have already been developed and tested with success by the laboratories involved in the project, in particular for texture and residual stresses, crystal structure and defect analysis.

T2.3: Testing and verification

The integrated approach will be tested initially on already existing machines easily adaptable to integration of some of the methodologies. For reflectivity and diffraction measurements these will be collected initially on different machines and the analysis performed using the integrated methodology. As the integrated instrument and analysis system will be available a more complete and real testing will be performed considering also efficiency of the approach in term of analysis speed, operator intervention and accuracy of the results. The tests will be performed on different film and structure systems, ranging from single layered to multilayered structures and spatial resolution. The methodology approach will be modified and tuned according to the results obtainable and the production monitoring needs.

T3.1: System layout definitions

The software system characteristic and the general layout following an object oriented (OO) approach will be defined. The layout design will take into account also the integration of existing methodologies already coded in available routines. These will need a radical modification to be suited for the OO layout. The main points of the layout design will be: easy of use, automation, database support, high portability and network integration, pluggable methodology and look and feel approach, extendibility, flexibility and customisation possibilities.

T3.2: GUI (Graphical User Interface) implementation and routine integration

The system will be implemented in Java, the only OO language available to meet the specifications. This will permit to construct a user friendly interface, not constrained to a particular computer hardware and with the possibility to run through the Internet. The Java virtual machine is also well suited for database support and for integration with already existing routines from different languages. The analysis system will be based on a combination of a non-linear least square fitting and entropy maximisation methodology where the film and material properties will be parameters to be refined until the computed and experimental data will be matching. The user will choose information needed and indicate the expected compounds present on the sample. If these are unknown, a faster early preview analysis can be performed to identify them. The initial composition and structure of the sample analysed can be implemented directly from the layout of the device.

T3.3: Testing and user customisation.

The program interface will be tested during development for methodology integration on different data and traditional machines. This early testing will be used mainly for methodology assessment. Subsequently after completion of the expert system, the software will be used for analysis of standard samples and advanced electronic films. The testing by the final user will permit a tuning of the user interface as well as an optimisation of the automatic and intelligent system of analysis. Testing on a wide variety of problems will be necessary for general assessment of the approach and learning process of the expert system. Tuning of the automatic analysis method will be based on the accumulating experience approach (similar in principle to a learning system, but not automatic).

T4.1: Instrument building

The basic elements for the instrument will be selected, assembled and tested to obtain the hardware part of the system. It will consist of a high precision goniometer equipped with an Eulerian open cradle suitable for mounting large sized specimens and scanning through the entire sample on a reduced spatial resolution. A collimator system to analyse macro-area (over 1 cm²) and micro-area (down to 100 microns² or less) will be mounted on the system. The detector will be a curved position sensitive detector with the ability to collect an entire spectrum of near 120 degrees in two-theta in less than a minute. The whole diffractometer will be completed with a high stability power generator, X-ray tube system and interfaces to remotely control the entire instrument. The special feature of the instrument will be the ability to collect a high number of spectra at different tilting and azimuths angles (determined by the expert system) in a reasonable time for diffraction and reflectivity analysis without moving or mount/unmount the sample or intervention of the operator.

T4.2: Expert system integration

The hardware and interface software developed will be integrated with the analysis software to minimise collection and analysis time, to allow automatisation of the whole measurement/analysis process, to obtain more information with high accuracy, to remotely control the process also through the internet, to reduce the dead-time of the system and to implement of a more user friendly system following human interface specifications.

T4.3: Installation and assessment

The instrument will be installed at the final user location. Early testing will be performed on some standard samples for assessment of overall quality and accuracy obtainable by the expert system. Hardware and mainly software will be optimised and tuned to better reflect the user needs or improve the overall quality and efficiency of the system.

T5.1 Silicides films will be prepared by Ti deposition (sputtering) and silicidization by rapid thermal annealing treatment. Deposition will be performed both in presence and absence of Mo on the silicon interface in order control phase formation of the silicide. Uniform films and test patterns of different sizes will be prepared. Samples will be qualified by electrical tests (spreading resistance).

T5.2 Aluminium and copper metallic films, homogenous films and test patterns will be prepared by sputtering (aluminium) or electroplating (copper). Film quality, thickness and uniformity will be tested by electrical resistivity measurements and by optical reflectivity. This samples will be obtained either from the production line or the pilot line of the IC manufacturer at regular intervals.

T5.3 Ferroelectric materials preparation and qualification

Preparation of ferroelectric thin films for pyroelectric IR detectors and non-volatile RAM memories will be carried out.

Ferroelectric thin films of modified lead titanate (MPT) and strontium bismuth tantalate (SBT) will be prepared by a novel sol-gel spin-coating procedure. Ferroelectric measurements such as hysteresis loops, switching current densities versus electric field, fatigue, retain, transition temperature, pyroelectric coefficients and leakage currents will be carried out to qualify samples. From these relations, the appropriate deposition parameters will be established for the fabrication of MPT and SBT thin films with a good performance in pyroelectric sensors and non-volatile memories.

T5.4 Thin silicon oxides films of thickness between 2.0 and 20.0 nm will be prepared by STMicroelectonics, with different techniques. For thickness below 5.0 nm preparation will be done by diluted steam oxidation in vertical furnaces with or without nitridation. Nitridation will be performed in cascade by annealing at high temperature in presence of N2O or NO. For very low thickness (below 3.0 nm) also rapid thermal oxidation (RTP) and rapid thermal nitridation (RTN) will be used. Above 5.0 nm oxidation will be performed by steam or dry oxidation at high temperature. Qualification of the preparation protocols for the thickness requested will be performed by ellipsometry.

T6.1 Film thickness measurements on ultra thin films. Thickness measurements will be done using the reflectivity configuration on silicon oxide thin films. Accurate estimation of thickness, roughness of surface and interface silicon-silicon oxide will be performed. As a control the samples will be sectioned and analysed with TEM and /or metallized and measured by Fowler Nordeim technique.

T6.2 Ferroelectric materials characterisation. The new system will be used to determine the structural phases of MPT and SBT films during their crystallisation. In both cases, the formation of second pyrochlore/fluorite-type phases deteriorates the electrical properties of the films. Also, reactions between the underlying substrate and the film lead to non-ferroelectric interfaces that also affects negatively the performance of these films. In the case of the MPT films, parameters of the deposition process will be changed to obtain the maximum orientation in the polar direction. MPT films will be deposited onto different substrates to promote preferred orientation. (100)SrTiO₃, (100)MgO and (100)Si substrates will be tested. Different thin inter-layers between the substrate and the ferroelectric film will be tested to improve orientation (Ti, TiO₂, Pt_xTi, …). Texture of the inter-layers will be also studied with the new X-ray system. For SBT films, parameters of the deposition process will be established to obtain the minimum alignment of the polar direction lying on the film plane. (100) Si substrates with platinum electrodes and different inter-layers will be tested. Stresses will be studied with the new expert X-ray system proposed. Films prepared by the sol-gel spin-coating technique develop a large amount of stresses that usually can be reduced by controlling the process parameters. However, in some cases stresses can favour the ferroelectric response of the films. MPT films with compressive stresses develop higher spontaneous polarisation and pyroelectricity. Also, changing the sign of the stresses in the SBT films, it is expected to increase the contribution of the polar axis along the perpendicular direction of the film. Thickness of the films will be also measured by the new system and compared with the results obtained from Profilometry measurements and regular reflectometry.

Correlation between structural phases/texture/stress/thickness of the films and ferroelectric properties will be carried out. Profilometry combined with the Stone´s expression will be used to determine stresses from the measurement of curvature of ferroelectric thin films and compared to the stresses obtained by the X-ray system.

T6.3: Silicides characterisation. X-Ray diffraction will be performed on silicides. In the first case the aim is to characterise the phase formed in TiSi₂ samples in presence/absence of Mo to assess the formation of the C54 against C49 phases. Samples will be TiSi₂ deposited in presence and absence of Mo with and without annealing. Raman will be used as a comparison technique in addition to conventional XRD.

T7.1 Metallisation characterisation. Structural phases, thickness, texture and stress-strain will be determined on aluminium and copper films obtained at regular intervals from production or pilot line in order to monitor film quality and performance over the time. Problems related to equipment malfunction or substrate cleanliness causing poor film quality (low texture, high stress, non uniform thickness, wrong crystalline phase), will be detected by the instrument.

The study will be done on homogenous films and on test patterns as well.

T7.2 New processes development. Support will be provided for new processes development of the IC manufacturer by characterising thin films produced with innovative technologies. Multilayered samples will be also considered. Problems encountered by processes engineers like adhesion problems induced by stress-strain, low film performances in terms of conductivity, dielectric constant, insulating capabilities, unknown phase formation at interfaces will addressed by means of a detailed description of film properties. This task will require an efficient communication flow between process engineers and people involved in the project. This will be granted by the physical proximity of the instrument with the pilot line, by the strong contacts already established between the characterisation laboratory and the process engineers and by frequent action taken by the project management to communicate project status, calls for problem solving requests, demonstration of instrument capabilities through seminars.

T8.1 Participation to scientific conferences. Oral and poster contributions will be submitted to conferences dedicated to X-Ray diffractometry and materials science in general.

T8.2 Participation to Semicon exposition. A brochure will be prepared and made available at the Semicon meetings with modalities to be defined.

T8.3 Organisation of a workshop. A workshop will be organised and potential users will be invited together with experts in X-Ray diffraction/reflectivity techniques. The topic of the workshop will be centred on thin films analysis.

T8.4 Distribution through web server of demo version of analysis software. A Web site will be set-up where interested people will be able to browse all the information regarding the project. A free version of the analysis software will be made available on the site as a running applet.

CONSORTIUM OVERVIEW FOR ANONYMOUS PART B
Participant		Business activity / Main Mission / Area of activity	RTD Role in project
Activity code 1	Nr.
REC	1	Applied research on microlectronics materials and devices	Principal contractor
IND	2	Manufacturer of Integrated Circuits	Principal contractor
HES	3	High education and research in materials engineering	Principal contractor
HES	4	High education and research in solid state phisics	Principal contractor
REC	5	Research on material science and technology	Principal contractor
IND	6	Manufacturer of diffractometers	Principal contractor
IND	7	Manufacturer of diffractometers	Principal contractor

OVERVIEW OF DELIVERABLES
Deliverable No1	Delivery date2	Output from W.P. Nr.	Nature of Deliverable3 and brief description
D1	3	2	Methodology. Optimum methodology to calculate phase composition
D2	3	2	Methodology. Optimum methodology to calculate texture
.D3	3	2	Methodology. Optimum methodology to calculate stress-strain
D4	3	2	Methodology. Optimum methodology to calculate film thickness
D5	3 -24	5	Materials. Ferroelectric thin films qualified.
D6	3 -24	5	Materials. Silicides thin films uniform and patterned
D7	3 -24	5	Materials. Silicon oxides of different thickness
D8	4	3	Layout. Software system layout definition with object oriented approach.
D9	5	4	Instrumentation. Hardware part of the instrument is built. Specifications are fulfilled.
D10	8	2	Methodology. Integrated methodology to simultaneously calculate all thin film properties.
D11	11	8	Web site set-up.
D12	12	4	Instrumentation. The software is able to control all the functionalities of the instrument and to acquire spectra in any configuration.
D13	12	3	Software. First beta release of off-line analysis software with all the functionality planned with an advanced GUI. Downloadable through Internet.
D14	13	2	Analysis. Test samples are extensively analysed, samples are correctly described in terms of phase composition, stress-strain, texture and thickness after the calculation with chosen algorithms.
D15	16	4	Software. Acquisition and analysis software are fully integrated. Computation algorithm detect missing data and drive further acquisition.
D16	18	3	Software. Stable release of the analysis software with improved GUI and algorithms. Downloadable through Internet.
D17	20	4	Software. Stable release of the acquisition-analysis software with improved GUI and algorithms
D18	20	4	Instrumentation. Instrumentation installation and assessment is completed.
D19	24	8	Workshop organisation
D20	26	6	Analysis. Thin silicon oxide films are characterised, and accurate layer thickness roughness is calculated and compared with TEM.
D21	27	6	Analysis. Ferroelectric films are fully characterised and texture stress-strain, phase composition, thickness are known. Data are compared with ferroelectric properties.
D22	27	5	Materials. Aluminium and copper films prepared and qualified
D23	28	6	Analysis. Silicides are characterised in terms of phase composition, texture and stress-strain. Data are compared with Raman and conventional XRD.
D24	28	6	Report. A chart comparing the new instrument with other, conventional techniques is made considering not only accuracy of information, but also industrial feasibility.
D25	29	7	Analysis. Aluminium and copper films are characterised in terms of phase composition, texture and stress-strain.
D26	29	7	Analysis. Problem solving in industrial processes is proved with samples provided by process engineers.

OVERVIEW OF MILESTONES
Milestone No1	Due date	Brief description of Milestone objectives	Decision criteria for assessment
M1	9	Thin film properties obtained from spectra collected on traditional instruments. This is the Mid-term assessment milestone.	Physical parameters of thin films are described correctly from X-ray analysis. The properties are confirmed from other physical measurements.
M2	20	Instrument is able to perform a full set of analyses.	It is possible to obtain complete description of thin films properties by the analysis with the new instrument. Measurement can be performed by a non-expert. The properties are confirmed from other physical measurements
M3	29	The instrument proved to be useful for application in microelectronics	Information where provided which where useful to improve processes. Information where obtained without help from experts in diffractometry. Time scale to obtain information was compatible with process implementation needs.

WORKPACKAGE DESCRIPTION
Workpackge Title: Project management		WP nr:1
Starting date: month nr. 0 Duration: 30 months		Total Effort (pers.m):15
Partners involved	R & D Task/Activity of Partner	Effort (pers.m):
REC 1	Project control and management	15
Objectives The aim of the project management activities will be to monitor the progress of the work to guarantee a successful outcome of the plan of the project in terms of the set goals. Key tasks. The co-ordinator will control and require from any workpackage the progress status according to the scheduled project. Description of work / tasks Planning: The stages of this proposal will have to be reviewed at intervals according to the progress throughout the project life cycle by setting goals and objectives and establishing time and resources, identifying major tasks and agreeing on a budget, setting up a team and appointing key staff. Scheduling: This will be strictly connected to the progress achieved. It will involve a detailed work program task by task, allocating appropriate resources (people, equipment, materials etc.) and assigning time and cost budgets. Activities will be sequenced according to the inter dependencies and resources at our disposal. Re-scheduling may very likely take place in the course of the project. Co-ordination and control: The cost and quality of the project plans (see progress report below) will be monitored. A major part of the project management activity will involve problem-solving by modifying plans. As tasks have been suitably scheduled (see above) this will involve co-ordinating task progress. A progress report to be presented every three months, structured as following: updated project progress plan (Gantt) showing planned progress against actual progress, planned future activities against expected future activities task progress table showing expected planned start/finish against actual or expected start/finish. Status will be given (early/on time/late/completed) for ongoing tasks or tasks completed in the last three months. deliverable progress table showing planned deliverable delivery dates against actual or expected. Status will be given (early/on time/late/delivered). resource usage table showing planned resource usage against actual resource usage.   Milestones and criteria The project reviews with the EU commission are the key milestones for the project management. They require a specific co-ordination activity from the management team in assuring the preparation of the agenda and contributions from the consortium to ensure that a clear picture of project progress is given. Interrelation with other workpackages Timely progress reports required from the other workpackages. Control and revision of scheduled work, resources and budget on a workpackage base.

WORKPACKAGE DESCRIPTION
Workpackge Title: Methodology development		WP nr: 2
Starting date: month nr. 0 Duration: months 13		Total Effort (pers.m):22
Partners involved	R & D Task/Activity of Partner	Effort (pers.m):
HES 3	Algorithm selection and integration	12
HES 4	Algorithm selection	8
IND 6	Instrument specifications	1
IND 7	Detector specifications	1
Objectives Selecting, integrating and testing algorithms best suited for Thin Films characterisation Description of work / tasks Definition of methodologies for film thickness measurements, phase composition characterisation, texture and stress-strain calculation. Integration of the algorithms selected to calculate simultaneously all the properties on multilayered structures. Testing of the mathematical procedures on spectra collected on already existing equipment. Deliverables D1, D2, D3, D4, D10, D14     Milestones and criteria Film thickness, texture, stress/strain and phase composition are calculated in a unique acquisition/analysis session.(M1). Interrelation with other workpackages Samples obtained from WP5

WORKPACKAGE DESCRIPTION
Workpackge Title: Expert system implementation		WP nr:3
Starting date: month nr. 0 Duration: months 18		Total Effort (pers.m):46
Partners involved	R & D Task/Activity of Partner	Effort (pers.m):
HES 3	Programming and testing	18
HES 4	Support in algorithm implementation, testing	12
REC 1	Software tester	2
IND 6	Programming support for instrumentation	7
IND 7	Programming support for detector	7
Objectives Developing a software capable to process X-Ray diffraction/reflectivity data and to deliver information on physical properties of mono/multilayered thin films usable by non experts. Description of work / tasks A layout of the software system will be defined following an object oriented approach. A Graphical user interface (GUI) will be implemented together with algorithms optimised in WP2. Software ability to deliver the information required, easiness to operate, stability of the system will be extensively tested.     Deliverables D8, D13, D16     Milestones and criteria The software is fully functional, stable easy to use. Acquisition and analysis are well integrated (M2) Interrelation with other workpackages Algorithms and data from WP2 will be implemented.

WORKPACKAGE DESCRIPTION
Workpackge Title: Instrument installation		WP nr: 4
Starting date: month nr. 0 Duration: months 20		Total Effort (pers.m):31
Partners involved	R & D Task/Activity of Partner	Effort (pers.m):
IND 6	Instrument assembling, software libraries for instrument control development.	10
IND 7	Position sensitive detector construction and adaptation to the new instrument. Software library for detector control.	10
HES 3	Software acquisition and analysis development and integration	4
REC 1	Instrument hosting and testing.	6
Objectives Producing a fully featured instrument for data acquisition and analysis easy to use, fast and reliable. Description of work / tasks The instrument will be assembled from commercially available components adapted and modified for the particular set-up desired. The instrument will be equipped with an innovative software interface with an expert system a database and an intuitive user interface. The instrument will be installed and extensively tested and improved and optimised for thin films analysis.         Deliverables D8, D13, D16   Milestones and criteria Instrument is fully functional, easy to operate, it delivers the desired information on an acceptable time scale (M2). Interrelation with other workpackages Implements software from WP3 it tests samples from WP5

WORKPACKAGE DESCRIPTION
Workpackge Title: Samples preparation and qualification		WP nr:5
Starting date: month nr. 2 Duration: months 26		Total Effort (pers.m):20
Partners involved	R & D Task/Activity of Partner	Effort (pers.m):
IND 2	Silicides, metals, oxides film preparation, electrical characterisation	6
REC 5	Ferroelectric film preparation and qualification	14
HES 4	Qualification measurements	10
Objectives Providing state of the art samples simulating with increasing degree of complexity real world microelectronics devices.. Description of work / tasks Ferroelectric materials made of MPT and SBT will be prepared by sol-gel spin-coating. Ferroelectric measurements will be carried out to qualify samples. Silicides preparation as homogenous and patterned films. Aluminium and Copper thin films preparation from the production lines. Silicon oxide ultra-thin films preparation. Every film will be qualified by testing electrical and optical properties.         Deliverables D5, D6, D7, D22     Milestones and criteria A complete set of samples chosen as probe is available. The samples are fully qualified and their preparation is reproducible. Physical properties under investigation such as thickness, stress/strain, texture are controllable and modifiable. Interrelation with other workpackages It will provide samples for WP2, WP4, WP6 and WP7

WORKPACKAGE DESCRIPTION
Workpackge Title: Analysis and comparison of qualified samples		WP nr:6
Starting date: month nr. 15 Duration: months 15		Total Effort (pers.m):36
Partners involved	R & D Task/Activity of Partner	Effort (pers.m):
REC 1	Novel instrument operation and testing. Raman measurements.	10
IND 2	Conventional X-Ray, TEM measurements, Fowler Nordheim	2
HES 3	Software tune-up and analysis support, microstructural analysis for comparison	4
HES 4	Consulting on algorithm tune-up	10
REC 5	Profilometry on ferroelectric.	10
Objectives To prove the usefulness of the instrument in a number of applications. To refine instrument performances and usability on the basis of user’s feedback. Description of work / tasks Silicides thin films and test pattern will be characterised. Phase composition, texture, stress/strain, thickness will be measured. Control measurements with Raman, conventional X-Ray diffraction and TEM will be used for comparison. Ferroelectric thin films made of MPT and SBT deposited on different substrates and layered structures will be characterised. . Phase composition, texture, stress/strain, thickness will be measured. Comparison will be made with profilometry and Raman. Thin silicon oxide film will be characterised in terms of film thickness, roughness and interface quality by the novel instrument. Control measurements will be carried out with TEM and Fowler-Nordheim. Producing an exhaustive analysis of benefit and problems deriving from utilisation of the novel instrumentation to characterise thin films properties.   Deliverables D20, D21, D23, D24     Milestones and criteria Sample provided by WP5 are fully characterised. Physical properties are measured and are comparable with the those obtained from the control techniques. Collection of data and analysis has been straightforward and doable by non-experts. Interrelation with other workpackages It utilise the outputs from WP3, WP4, WP5.

WORKPACKAGE DESCRIPTION
Workpackge Title: Problem solving of process engineering		WP nr: 7
Starting date: month nr. 20 Duration: months 10		Total Effort (pers.m):10
Partners involved	R & D Task/Activity of Partner	Effort (pers.m):
REC 1	Novel instrumentation operation, comparison measurements.	7
IND 2	Problems proposers, sample preparation, electrical measurements	2
HES 3	Methodology and analysis support	1
Objectives Demonstrate the capabilities of the novel technique in solving processes related problems. Description of work / tasks Aluminium and copper thin films be characterised. Phase composition, texture, stress/strain, thickness and roughness will be measured. Thin film quality will be assessed. Problems arising from development of new technologies and to production will be approached by the novel technique to demonstrate capabilities of then instrument for quality control.   Deliverables D25, D26     Milestones and criteria The novel technique proved to give exhaustive and accurate description of thin films properties and an effective problem solving tool in production and new material development (M3). Interrelation with other workpackages It utilise the outputs from WP3, WP4, WP5.

WORKPACKAGE DESCRIPTION
Workpackge Title: Dissemination		WP nr: 8
Starting date: month nr. 9 Duration: months 30		Total Effort (pers.m):29
Partners involved	R & D Task/Activity of Partner	Effort (pers.m):
REC 1	Participation to conferences / papers publication/ Web site	2
IND 2	Participation to Semicon	1
HES 3	Web server / Participation to conferences/ papers publication	6
HES 4	Participation to conferences/ papers publication	4
REC 5	Participation to conferences/ papers publication	4
IND 6	Workshop organisation, advertisement	6
IND 7	Workshop organisation, advertisement	6
I Objectives Giving adequate visibility to the project to assure that the achievements of the project contribute to economical and social growth. Description of work / tasks Spreading scientific knowledge accumulated during the project to the scientific community through participation to conferences and publication of papers. Inform potential new users of the capabilities of the new technique through a Workshop organisation, a Web site/server and the participation to Semicon meeting.   Deliverables D19   Milestones and criteria Potential new users have been adequately informed of the achievements of the project and the benefits of adopting the novel technique. The scientific results obtained have been transmitted to the scientific community, the part of the free software has been made available to people interested in the technique. Interrelation with other workpackages It utilise outputs from WP2, WP3, WP4, WP5, WP6 and WP7

Title *

Table of content *

C3 - Contribution to objectives of Programme/Call *

C4 - Community Added Value and contribution to EU Policies *

C5 - Contribution to Community Social Objectives *

C6 - Economic Development and S&T prospects *

C7 The consortium *

C8.1. Project management *

C9 List of references and related projects *

0. The proposed approach to the determination of thin films properties answers the need of new measurements and testing tools. Such need is particularly significant in microelectronic industry where the requirements for improved miniaturisation and device performances are pushing towards more sophisticated measuring instrumentation.
1. This project has the following objectives:

1. To set a new standard in thickness measurements for thin films in the range of few nanometers where ellipsometry is no longer a feasible technique, by means of a user-friendly instrument able to perform measurements on a routinary basis for quality control.
2. To provide a tool able to monitor in a quantitative manner the quality of thin films by measuring in parallel a set of important properties. People without experience in this technique will be able to obtain detailed information on thin films properties, easing processes of optimisation and control.
3. To meet the new standard procedures and contribute to the standardisation initiative on the field of non-destructive testing: X-ray diffraction measurements under development through the CEN normative.

0. The results of the project will be:

• an expert system able to overcome the limitations imposed by the existing instrumentation. It will be easy to use and user friendly to allow people with different competence to take advantage from information provided by this technique. The final result will be a prototype constituted by a diffraction instrument equipped with an intelligent software dedicated to inspection of thin films and prevision of anisotropic properties;
• A new tool based on X-ray diffraction/reflectivity for the non-destructive measurement market that will provide an improvement in the measurement accuracy, physical material characteristics as direct output and that will be friendly usable with a short learning curve;
• A new methodology standard for thin film analysis by X-ray diffraction/ reflectivity.

1. Exploitation of results will be possible in short term the prototype realisation and use. The instrumentation will bring a new tool in the market of microelectronic industry on a short term with results for market penetration on a medium term. The methodology improvement and dissemination, especially for standardisation purposes, will require a medium to long time for the full exploitation of results on a large basis.

0. The high scientific and technical problems connected to the exploitation of the project results could be solved only by a team of experts that actually cannot be located in a unique country inside the EU. It requires not only the knowledge and experience in the measurement/instrument construction field but also a strong background in the diffraction/reflection research ranging from basic crystallography to texture and residual stresses. A strong knowledge of the materials and thin film systems is required for the physical properties computation and to focus the tool to be implemented in the more efficient way with respect to the user needs. The success of the project strongly depends in an effective synergy between instrument builder and manufacturers, methodology experts and software developers, measurement and analysis experts and microelectronic users. As reported in the chapter "description of the consortium" the partners in this project will cover the necessary knowledge, know-how and resources but are distributed over three countries.
1. Even if the actual knowledge and technological level allows the realisation of a true expert system for electronic thin film research and quality control, these resources are distributed in different laboratories and factories of the EU. Again, the development of the expert system requires not only a construction of the instrument itself but a strong investment of human, laboratory and material resources to implement the methodology and analysis part, for assessment of the procedure and true integration between the tool features and the user needs in term of intelligent analysis, easy of use, suitability for quality control, effective usefulness of the output results (physical properties instead of meaningful unknown parameters).
2. The development of such system and methodology for quality and analysis control of microelectronic film products may lead to advantages in the following:

• help the EU microelectronic industry (ST in a shorter time) to reach the excellence target for improved competitiveness respect to the US and Japan leadership on the market;
• as a consequence there is an indirect advantage for an employment growth in the sector;
• opening of a new market concerning the non destructive quality control of electronic films by this expert tool; diffraction is used only as a research tool in this field at the moment;
• the lower requirement of human resources for measurement and analysis of data will permit to researchers to concentrate their effort in more strategic tasks without involvement in routinary work;
• the better precision and accuracy attainable will lead to an improvement of production quality standards;
• the easy of use and less requirement in term of basic and advanced knowledge of the diffraction/texture/reflectivity field will reduce the training of personnel and enlarge the applicability of the system;
• the characteristics of the system permit a better integration of the design, production and control steps leading to a sensible reduction of the time to market that it’s of great strategic importance in the electronic industry;
• the better understanding of the film properties will permit an improvement of the electronic devices advantaging the European electronic industry;
• the non-destructive nature of the analysis will lower the material consumption both at the research and quality control level;
• the instrument will integrate more techniques in one optimising and reducing the clean room space occupancy reducing cost and allocated resources.

The development of such a system will permit to investigate on new performance in X-ray multi-channel detector, optics and interfacing. This will imply to charge two new tasks for several months of engineers (electronics, optics and computation). In more the development will permit to work with sub-contractors (machining and electronics). The control of the achievement of this part of the project will be done by an engineer and a technician at Inel.

The principal objective of the project will be the realisation of this expert system for non destructive testing of thin electronic film. This will lead to a less consumption of material of high added value with consequence reduction also of the energy required for the device production.

Another point addressed by the project is the optimisation of the measurement time and the reduce totaltime for measurement by the position sensitive detector. All these requirements are consistent with an less energy consumption respect to the traditional apparati.

The project is classified as an X-ray diffractometer. A safety device must agree with the European description on X-ray radiation protection. There is no exhaust or polluting parts. Detectors requires a gas tank composed by a mixture of Ar-Ethane. Particular attention will be played to maintain the consumption very low and on recycling of the gas. The water cooling system of the X-ray source can be connected to a water chiller.

The main exploitation plans are reported in the following table 1.

EXPECTED RESULTS AND EXPLOITATION
Project output/ Result	Range of Applications	Expected Impact	Timing	Partner(s) responsible for exploitation
Community Added Value:
Better control of thin film production	Microelectronic devices	Most of the microelectronic industries	medium	STM MDM
Better understanding of thin film properties	Microelectronic devices	Most of the microelectronic industries	long	STM MDM CSIC
Reduced time for research development and new product design and optimisation	Microelectronic devices, Structural material production (composites), Biomedical applications	Most of the microelectronic ad advanced materials production industries	medium	STM MDM CSIC
Social / Environmental Impact:
Automatisation of X-ray analyses Reduced risk for X-ray contact	Any X-ray diffraction laboratory (public and industry)	large	long	IS UNITN LPEC
Reduced material consumption for testing/control	Only high costs materials and devices	Microelectronic industry	short	STM MDM CSIC
Technical / Economic Impact:
X-ray Expert system	Quality control of: thin films microelectronics advanced materials	restricted to: microelectronic industry, research laboratories, market to be created	medium	IS
Optimisation of thin film texture	Improved efficiency of devices and material parts	microelectronic industry, advanced material production industry	medium	STM

For a long time, X-ray diffraction have been a tool for fundamental research. Since the last ten or fifteen years, industry have found an interest in the technics to identify and to quantify chemical phases. Then the control of production can easily be done in many fields such as pharmacy, cement, mining, electronics, metallurgy …

The actual high technicality of new materials requires new kind of measurements (texture, stress, reflectometry, diffusion …), and which are performed in highly specialized laboratories. Actually a new need is often asked by industry to get such information. Then the need of an Expert goniometer is growing, and such equipment does not really exist at the scale of earth. Consequently, the market is new, and the spreading is large. This Expert instrument developed with a European knowledge and know-how could be sale in the world wide. Our sale subsidiary in USA can be stepping stone of the new European Expert goniometer. This can only be achieve by sharing the knowledge in instrumentation and sciences. We believe that such an apparatus would give such a competitive edge to the work of any manufacturer that eventually all of them would have to buy one. The market for this apparatus is in semiconductor manufacturers and research laboratories doing research into semiconductor and other thin films. We anticipate being able to sell about three per year for the seven years year following the successful completion of the project.

C7 The consortium